高效液相色谱-串联质谱法测定鱼肉中3种微囊藻毒素

Determination of Three Microcystins in Fish by High Performance Liquid Chromatography Tandem-Mass Spectrometry

本文建立了一种测定鱼肉中3种微囊藻毒素的方法样品用甲醇溶液提取后,经C18固相萃取柱净化后,采用高效液相色谱-串联质谱仪测定,外标法定量在0.2〜5.0μg/L浓度范围内,微囊藻毒素RR、微囊藻毒素YR和微囊藻毒素LR有良好的线性关系,线性相关系数均大于等于0.999,定量限均在0.2μg/kg以内。考察了空白鱼类样品添加3个浓度水平的回收率结果,样品中微囊藻毒素RR、YR和LR的回收率分别为95.0%〜96.5%、93.0%~102%和88%~101%,RSD在4.41%以内。

A method for the determination of three microcystins in fish was developed in this paper.The samples were extracted with methanol and purified by C18 SPE column,with high performance liquid chromatography tandem mass spectrometry for determination and external standard method for quantification.The method showed good linearities when the concentration of microcystin RR,microcystin YR and microcystin LR ranged from 0.2〜5.0μg/L,the correlation coefficients were ei or equal to 0.999,and the limits of quantitation were all within 0.2μg/kg.Three different concentration levels of microcystin RR,YR and LR were added in fish samples,the recovery rates of microcystin RR,YR and LR were between 95.0%〜96.5%,93.0%〜102%and 88%~101%respectively,and the RSDs were within 4.41%.